Hierarchical In 2 O 3 @WO 3 nanocomposites, consisting of discrete In 2 O 3 nanoparticles (NPs) on singlecrystal WO 3 nanoplates, were synthesized via a novel microwave-assisted growth of In 2 O 3 NPs on the surfaces of WO 3 nanoplates that were derived through an intercalation and topochemical-conversion route. The techniques of XRD, SEM, TEM and XPS were used to characterize the samples obtained. The gas-sensing properties of In 2 O 3 @WO 3 nanocomposites, together with WO 3 nanoplates and In 2 O 3 nanoparticles, were comparatively investigated using inorganic gases and organic vapors as the target substances, with an emphasis on H 2 S-sensing performance under low concentrations (0.5-10 ppm) at 100-250 C. The results show that the In 2 O 3 NPs with a size range of 12-20 nm are uniformly anchored on the surfaces of the WO 3 nanoplates. The amounts of the In 2 O 3 NPs can be controlled by changing the In 3+ concentrations in their growth precursors. The In 2 O 3 @WO 3 (In/W ¼ 0.8) sample has highest H 2 S-sensing performance operating at 150 C; its response to 10 ppm H 2 S is as high as 143, 4 times higher than that of WO 3 nanoplates and 13 times that of In 2 O 3 nanocrystals. However, the responses of the In 2 O 3 @WO 3 sensors are less than 13 upon exposure to 100 ppm of CO, SO 2 , H 2 , CH 4 and organic vapors, operating at 100-150 C. The improvement in response and selectivity of the In 2 O 3 @WO 3 sensors upon exposure to H 2 S molecules can be attributed to the synergistic effect of In 2 O 3 NPs and WO 3 nanoplates, hierarchical microstructures and multifunctional interfaces.